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A method for adsorption and purification of tungsten hexafluoride

A technology of tungsten hexafluoride and adsorbent, which is applied in the field of purification, can solve the problems of difficult separation and the adsorption effect is difficult to reach the volume content of tungsten hexafluoride gas, and achieve the effect of improving the capacity

Active Publication Date: 2017-06-13
ZHEJIANG BRITECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Tungsten hexafluoride gas purification method in the prior art, MoF 6 The melting point and WF 6 The boiling point of tungsten hexafluoride is close to, and it has a higher vapor pressure near the melting point, so it is difficult to separate, and the adsorption effect is difficult to reach the level of 99.99% of the volume content of tungsten hexafluoride gas

Method used

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  • A method for adsorption and purification of tungsten hexafluoride

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Step 1. Load operation:

[0019] In a 1000L reactor, add 100Kg fluorinated carbon fiber, 1Kg nickel chloride, 400Kg N,N-dimethylformamide, 1Kg 1-vinyl-3-ethylimidazole hexafluorophosphate, and react at 60°C for 15 hours. After standing still for 40 hours, 1Kg of 5,10,15,20-tetrakis(4-pyridyl)porphyrin was added, reacted at 60°C for 15 hours, and the product was separated and dried to obtain the adsorbent.

[0020] Step 2. Adsorption and purification of tungsten hexafluoride:

[0021] Under the conditions of 40°C and 0.5MPa, industrial-grade tungsten hexafluoride is adsorbed in a chromatographic column equipped with adsorbent at a flow rate of 3BV / h to obtain tungsten hexafluoride product. The purity of tungsten hexafluoride is shown in Table 1, and the code is M-1.

Embodiment 2

[0023] Step 1. Load operation:

[0024] In a 1000L reactor, add 100Kg fluorinated carbon fiber, 0.5Kg nickel chloride, 200Kg N,N-dimethylformamide, 0.5Kg 1-vinyl-3-ethylimidazole hexafluorophosphate, and react at 50°C After 10 hours, stand still for 20 hours, then add 0.5Kg of 5,10,15,20-tetrakis(4-pyridyl)porphyrin, react at 40°C for 10 hours, separate and dry the product to obtain the adsorbent.

[0025] Step 2. Adsorption and purification of tungsten hexafluoride:

[0026] Under the conditions of 10°C and 0.2MPa, industrial-grade tungsten hexafluoride is adsorbed in a chromatographic column equipped with adsorbent at a flow rate of 1BV / h to obtain tungsten hexafluoride product. The purity of tungsten hexafluoride is shown in Table 1, and the code is M-2.

Embodiment 3

[0028] Step 1. Load operation:

[0029] In a 1000L reactor, add 100Kg fluorinated carbon fiber, 2Kg nickel chloride, 500Kg N,N-dimethylformamide, 2Kg 1-vinyl-3-ethylimidazole hexafluorophosphate, and react at 80°C for 24 hours. After standing still for 60 hours, 2Kg of 5,10,15,20-tetrakis(4-pyridyl)porphyrin was added, reacted at 80°C for 20 hours, and the product was separated and dried to obtain the adsorbent.

[0030] Step 2. Adsorption and purification of tungsten hexafluoride:

[0031] Under the conditions of 70°C and 1MPa, industrial-grade tungsten hexafluoride is adsorbed in a chromatographic column equipped with adsorbent at a flow rate of 5BV / h to obtain tungsten hexafluoride product. Numbered M-3.

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Abstract

The invention relates to a method for adsorbing and purifying tungsten hexafluoride.The method comprises the steps of adding fluorinated carbon fibers into a reaction kettle, and conducting on-load operation, so that adsorbent is obtained; adsorbing industrial-grade tungsten hexafluoride with a chromatographic column filled with the adsorbent, so that a tungsten hexafluoride product is obtained.

Description

technical field [0001] The invention relates to a purification method, in particular to a method for adsorbing and purifying tungsten hexafluoride. Background technique [0002] In tungsten fluoride, WF 6 It is the only variety that is stable and industrially produced. Its main use is as a raw material for metal tungsten chemical vapor deposition (CVD) process in the electronics industry, especially WSi made of it 2 Can be used as wiring material in large scale integration (LSI). The composite coating of tungsten and rhenium is prepared by the CVD process of mixed metals, which can be used in the manufacture of X-ray emitting electrodes and solar absorbers. In addition, WF 6 In the electronics industry, it is also mainly used as a raw material for semiconductor electrodes and conductive pastes. [0003] WF 6 There are also many non-electronic applications. For example, tungsten can generate hard tungsten carbide on the surface of steel by CVD technology, which can be u...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G41/04
CPCC01G41/003C01G41/04
Inventor 陈刚贺辉龙李军张晓东张广第周井森王琪宇王新
Owner ZHEJIANG BRITECH CO LTD
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